Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3-Methoxyacetophenone → 1-(3-Methoxyphenyl)-2-(1-methyl-2-pyrrolidinyliden)ethanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3-Methoxyacetophenone | HCID 11460 | — |
| 반응물 | Sodium | HCID 5360545 | — |
| 반응물 | 2-Dimethylamino-1-methyl-1-pyrrolinium methylsulfate | HCID 178483037 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 1-(3-Methoxyphenyl)-2-(1-methyl-2-pyrrolidinyliden)ethanone | HCID 57153745 | 60.2% |
반응 단계
A solution of 10.35 g of sodium in 225 ml of ethanol is added dropwise at 90° (with stirring) in the course of one hour to a mixture of 107 g of 2-dimethylamino-1-methyl-1-pyrrolinium methyl sulfate and 45.1 g of 3-methoxyacetophenone; stirring is effected for a further 2 hours at this temperature, and the solvent is then largely distilled off under a vacuum. 300 ml of water and 300 ml of diethyl ether are added to the cooled residue, and thorough shaking is effected. The ethereal phase is collected, dried over sodium sulfate and concentrated. The crystalline residue is recrystallized from chloroform/cyclohexane to yield 41.8 g of the title compound (as yellowish crystals), m.p. 92° to 93°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04198424 |
| 출처 데이터셋 | uspto-grants-1980_04 |
| ORD ID | ord-35e91b2a19d649d69cdd896ca81c5f02 |
| 출처 메모 | uspto-grants-1980_04 |